US5155340A - Thin high temperature heater - Google Patents
Thin high temperature heater Download PDFInfo
- Publication number
- US5155340A US5155340A US07/550,976 US55097690A US5155340A US 5155340 A US5155340 A US 5155340A US 55097690 A US55097690 A US 55097690A US 5155340 A US5155340 A US 5155340A
- Authority
- US
- United States
- Prior art keywords
- adhesive layer
- high temperature
- heater
- group
- thin high
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/13—Solid thermionic cathodes
- H01J1/20—Cathodes heated indirectly by an electric current; Cathodes heated by electron or ion bombardment
- H01J1/22—Heaters
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
- H01J9/08—Manufacture of heaters for indirectly-heated cathodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2201/00—Electrodes common to discharge tubes
- H01J2201/28—Heaters for thermionic cathodes
- H01J2201/2803—Characterised by the shape or size
- H01J2201/2878—Thin film or film-like
Definitions
- the present invention relates to a small heater for heating to high temperature and a manufacturing method therefor and, more particularly, to a thin heater for heating to high temperature such as a heater for an electron gun, a hot cathode X-ray tube, a Braun tube and so on which is used at approximately 1000° C. and a manufacturing method therefor.
- FIG. 3 is a sectional view showing a cathode of an electron tube using a conventional heater.
- reference numeral 10 designates a ceramic substrate
- reference numeral 11 designates a heating element layer
- reference numeral 12 designates an insulating layer
- reference numeral 13 designates a cathode lead layer
- reference numeral 14 designates a base metal layer
- reference numeral 15 designates a cathode material layer.
- a raw material for forming the ceramic substrate 10 is prepared and then the heating element layer 11 having a desired pattern is formed on a sheet by a printing technique such as an extrusion method by which a material is extruded between rollers or a casting method.
- the heating element layer 11 is formed on the ceramic substrate 10 by screen printing a paste in which baking assistant is added to a heater agent. Thereafter, it is baked at high temperature (1000 ⁇ 2000° C.) and then the plane type heater is completed.
- FIG. 4 includes sectional views showing manufacturing steps for forming a conventional plane thin type heater by a thin film forming method.
- a resistor film for a heater 3 usually formed of metal such as tungsten is uniformly formed on a plane ceramic substrate as an insulating material a desired pattern is formed by etching, a lead wire (not shown) is connected thereto, and finally the plane type thin heater is completed.
- the adhesion between the resistor film 3 for the heater and the insulating material 1 is small. Therefore, in order to increase the adhesion between the resistor film 3 and the insulating material 1, an adhesive layer is used.
- a Ti film with a thickness of several tens to several hundreds of nanometers (nm) is formed as the adhesive layer and then the resistor layer is formed thereon to provide the thin high temperature heater.
- the heater is used with a voltage applied thereto, that is, when a high temperature load of 1000° C. is applied, Ti is degraded, causing the heater to break down.
- FIG. 6 shows the SEM photograph of a heater in a breakdown state (where 20.0KV is an accelerating voltage of the scanning electron microscope, ⁇ 350 is a magnifying factor of 350, and a length of the line indicated corresponds to 100 microns).
- the reason for the breakdown is believed to be the transformation point of Ti from ⁇ to ⁇ phase (referred to as a transformation point hereinafter) at 882° C. and this transformation point is repetitively passed through while the heater is used.
- the resistance of the thin film resistor changes while it is used.
- FIG. 5 shows a change of resistance value with lapse of time. The reason why the resistance is reduced in an early stage is that recrystallization occurs in the thin film and then the size of the crystal grains in the thin film increase.
- the resistor heatsink
- W tungsten
- the temperature of 1000° C. corresponds to the recrystallization temperature of W
- recrystallization occurs.
- the reason why the resistance increases with lapse of time is that an impurity is mixed into the film or the film is oxidized by the ambient in use.
- the insulating substrate of an oxide group such as Al 2 O 3 is available in its monocrystalline state and a surface thereof can be mirror-finished, its pattern precision thereof is better than sintered substrates such as SiC, and AlN. Therefore, Al 2 O 3 has been conventionally used as the insulating substrate (insulating material) of the conventional thin film high temperature heater manufactured by the thin film forming method.
- FIGS. 7 and 8 are scanning electron microscope photographs showing two ends of a damaged heater.
- the conventional thin high temperature heater formed by the thin film forming methods is unstable as a heater and also unreliable as far as a long term use is concerned.
- the present invention was made in order to solve the above problems and it is an object of the present invention to provide thin high temperature heater with a high reliability in which adhesion between a resistor film for a heater and an insulating material is high and a resistance change is small.
- a thin high temperature heater comprises an adhesive layer comprising Ti formed on an insulating material and a resistor layer comprising a Ti compound formed on the adhesive layer.
- the Ti film increases adhesion between the insulating material and the resistor layer and the resistor layer is stable at high temperature as compared with a heater formed of metal because a Ti compound such as TiC, TiN or TiCN or a mixture thereof for the resistor layer is ceramic. Furthermore, even if Ti diffuses into the resistor layer while the heater is used, no deterioration occurs and the adhesive layer is stable because the resistor layer also comprises Ti.
- an adhesive relaxation layer comprising a TiC, TiN or TiCN or a mixture thereof and having a superior stability at high temperature is provided between the adhesive layer and the heating element. Therefore, adhesion between the heating element and the insulating material is high and Ti of the adhesive layer does not diffuse into the heating element. Furthermore, the heating element and the insulating material are not damaged by the interaction therebetween.
- a method for manufacturing the thin high temperature heater in accordance with the present invention comprise the step of forming an adhesive layer comprising Ti on an insulating substrate and a resistor layer comprising a Ti compound at temperature below the transformation point of ⁇ to ⁇ phase of Ti or forming them at temperature of the transformation point or higher.
- the adhesive layer and the resistor layer are formed a temperature below the transformation point or at temperature of the transformation point or higher, Ti is not degraded by high temperature while the heater is manufactured. More specifically, when they are formed at temperature below the transformation point, Ti is not transformed from ⁇ to ⁇ phase while the heater is manufactured, with the result that degradation is not likely to occur because of a change of volume. When they are formed at the temperature of the transformation point or higher, since Ti from the adhesive layer diffuses while the heater is manufactured, even if it is used thereafter at the temperature of the transformation point or higher, degradation by high temperature caused by the ⁇ to ⁇ transformation of Ti does not occur.
- FIG. 1 is a sectional view showing a thin high temperature heater in accordance with an embodiment of the present invention
- FIG. 2 illustrates a general etching process which is a part of manufacturing process for the thin high temperature heater shown in FIG. 1;
- FIG. 3 is a sectional view showing a cathode of an electron tube using a conventional thin high temperature heater
- FIG. 4 are views showing manufacturing steps for the conventional thin high temperature heater
- FIG. 5 is a graph showing a change of resistance value in the conventional thin film with lapse of time
- FIG. 6 is a scanning electron microscope photograph showing a heating element of a conventional thin high temperature heater, which is degraded by Ti at high temperature;
- FIGS. 7 and 8 are scanning electron microscope photograph showing two ends of a damaged heater in the plane type thin heater using a conventional oxide insulating substrate.
- FIG. 9 is a sectional view showing a thin high temperature heater in accordance with another embodiment of the present invention.
- FIG. 1 is a sectional view showing a thin high temperature heater in accordance with an embodiment of the present invention.
- reference numeral 1 designates an insulating material
- reference numeral 2 designates a Ti layer serving as an adhesive layer to the insulating material
- reference numeral 3 designates a resistor layer comprising a Ti compound of TiC, TiN or TiCN or a mixture of them and formed on the adhesive layer 2.
- the insulating material it is desirable that the insulating material have good heat conductivity a thermal expansion coefficient close to that of the resistor layer 3 be a good insulator, not break down at high temperature, and is planar. Therefore, in view of availability, it may be AlN, Al 2 O 3 or the like.
- a material of the adhesive layer 2 it is not particularly limited if it increases adhesion between the resistor layer 3 and the insulating material 1.
- a metal such as Ti, V, Cr, Y, La, Zr, Nb or Hf which has a thickness of 10 nm or less may be used and particularly Ti having the above thickness is most preferable among them because it is highly adhesive between the heating element 4 and the insulating material 1.
- the thickness of Ti exceeds 10 nm, degradation by high temperature occurs after repetitive use above the transformation point of Ti, which could cause a heater to break down.
- the resistor layer 3 is formed of a Ti compound such as TiC, TiN or TiCN or a mixture of them is that it has high recrystallization temperature and it has high electrical stability at high temperature.
- a general heater material such as W or Mo may be used.
- W or Mo may be used.
- such general heater materials take oxygen (deoxidizes) from the substrate 1 and form an oxide having high vapor pressure and scatter when this is formed on, for example, an Al 2 O 3 substrate 1 and used at a temperature of approximately 1000° C. More specifically, the resistor layer is etched away so that its configuration deforms. Therefore, it is stable while used as a heater, if the ambient or temperature is limited.
- a Ti film having a desired thickness is uniformly formed on the Al 2 O 3 substrate at 200 ⁇ 300° C. by sputtering. Then, it is etched to leave a desired pattern configuration by wet or dry etching. In case of wet etching, the etching is performed through the general steps as shown in FIG. 2.
- a sample having the pattern is arranged in a vacuum chamber for nitriding and then nitriding is performed below the temperature of transformation point of Ti, for example 400 ⁇ 500° C. and then N is diffused from the Ti surface. As a result, TiN is formed.
- Nitriding is performed to produce a layer which contributes to the adhesion between Ti and Al 2 O 3 at an interface with the substrate (10 nm or less).
- the depth of TiN is approximately several microns to 10 microns. If the nitriding is performed using a DC power supply, the Al 2 O 3 insulating material is not damaged and only the electrically conductive Ti is nitrided.
- the Ti film by sputtering is described in the above embodiment, that it may be formed by a PVD method such as an electron beam deposition method, a laser PVD method or an ion plating method.
- a PVD method such as an electron beam deposition method, a laser PVD method or an ion plating method.
- the pattern of Ti is formed and then nitriding is performed in the above embodiment, the same effect can be obtained even if nitriding is performed after the Ti film is formed and then the film is etched away by hot nitric acid or the like.
- TiC, TiN or TiCN or a mixture thereof may be formed by carbonization using a mixture of CH 4 and N 2 .
- the Ti film is formed and then nitriding or carbonization is performed at a surface before or after patterning.
- a second method will be described in reference to one example.
- a pattern mask is put on the Al 2 O 3 substrate heated to the desired temperature which is the transformation point of Ti or less, for example 200 ⁇ 300° C., and then a Ti film is formed by a normal Ar sputtering method.
- N 2 gas is introduced into the sputtering atmosphere and a TiN film having a desired thickness (several microns to 10 microns) is formed by reactive sputtering.
- TiC, TiN or TiCN or a mixture thereof is formed by changing the introduced gas to a gas comprising carbon, for example a mixture of CH 4 and N 2 .
- different films are continuously formed, for example Ti and then TiN during the process for forming the film.
- the thus manufactured thin type high temperature heater is not likely to be degraded by a change of volume because the adhesive layer and the resistor layer are both formed at a temperature which is below the transformation point of Ti and the transformation from ⁇ to ⁇ phase of Ti does not occur while the heater is manufactured.
- the adhesive layer is stable.
- a plurality of thin high temperature heaters in accordance with the second method may be formed on the substrate.
- a stable layer can be formed of a material which a low vapor pressure and stable electrical characteristic at a high temperature, such as W or Mo, on the insulator layer of the thin high temperature heater formed in accordance with the second method, as shown in FIG. 9, and then this can be used as the heating element.
- the resistor layer functions as an adhesive relaxation layer which prevents Ti of the adhesive layer from diffusing into the heating element.
- the adhesive layer and the resistor layer are both formed at a temperature below the transformation point of Ti in the above embodiment, they may be both formed at the temperature of the transformation point of Ti or higher. In this case, since the Ti for the adhesive layer is diffused in the manufacturing process, even if it is used at the temperature of the transformation point or higher, for example 1000° C., high temperature degradation caused by the ⁇ to ⁇ phase transformation of Ti does not occur.
- a thin high temperature heater comprises an adhesive layer comprising Ti and formed on an insulating material and a resistor layer comprising a Ti compound and formed on the adhesive layer.
- an adhesive relaxation layer comprising TiC, TiN or TiCN or a mixture thereof and having superior stability at a high temperature is disposed between the adhesive layer and the heating element. Therefore, adhesion between the heating element and the insulating material is high and Ti of the adhesive layer does not diffuse into the heating element. Furthermore, the heating element and the insulating material are not damaged by the interaction therebetween.
- the adhesive layer comprising Ti and the resistor layer comprising the Ti compound are formed on the insulating substrate, those layers are both formed at a temperature below the transformation point of ⁇ to ⁇ phase of Ti or both are formed at temperature of the transformation point or higher. As a result, Ti is prevented from being degraded by high temperature while the heater is manufactured.
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Resistance Heating (AREA)
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP1181016A JPH0343985A (ja) | 1989-07-12 | 1989-07-12 | 薄型高温ヒータおよびその製造方法 |
JP1-181016 | 1989-07-12 | ||
JP18685889A JP2752706B2 (ja) | 1989-07-18 | 1989-07-18 | 薄型高温ヒータ |
JP1-186858 | 1989-07-18 |
Publications (1)
Publication Number | Publication Date |
---|---|
US5155340A true US5155340A (en) | 1992-10-13 |
Family
ID=26500350
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US07/550,976 Expired - Fee Related US5155340A (en) | 1989-07-12 | 1990-07-11 | Thin high temperature heater |
Country Status (3)
Country | Link |
---|---|
US (1) | US5155340A (fr) |
EP (1) | EP0408342B1 (fr) |
DE (1) | DE69022651D1 (fr) |
Cited By (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5539186A (en) * | 1992-12-09 | 1996-07-23 | International Business Machines Corporation | Temperature controlled multi-layer module |
US5569474A (en) * | 1994-06-06 | 1996-10-29 | Daiho Industrial Co., Ltd. | Mold for injection molding of plastics using thin film electric heater |
US5616423A (en) * | 1994-05-19 | 1997-04-01 | Sumitomo Metal Industries, Ltd. | Ceramic substrate having a multilayered metallic thin film |
US5705272A (en) * | 1994-04-25 | 1998-01-06 | Canon Kabushiki Kaisha | Heating member and heat fixing apparatus using the same |
US5990449A (en) * | 1993-11-04 | 1999-11-23 | Pentel Kabushiki Kaisha | Electric heating device for mirror |
US6305923B1 (en) | 1998-06-12 | 2001-10-23 | Husky Injection Molding Systems Ltd. | Molding system using film heaters and/or sensors |
US6667100B2 (en) | 2002-05-13 | 2003-12-23 | Egc Enterprises, Inc. | Ultra-thin flexible expanded graphite heating element |
US20040056321A1 (en) * | 2002-06-28 | 2004-03-25 | Heetronix | Stable high temperature sensor system with tungsten on AlN |
US20040099047A1 (en) * | 2002-11-25 | 2004-05-27 | Raisanen Walfred R. | Thin film gas sensor |
US20040112892A1 (en) * | 2002-12-14 | 2004-06-17 | Abbott Richard C. | System and method for heating materials |
US6886233B2 (en) | 2002-05-13 | 2005-05-03 | Egc Enterprises, Inc. | Method for decreasing the thickness of flexible expanded graphite sheet |
US20050274714A1 (en) * | 2004-06-14 | 2005-12-15 | Hongy Lin | In-line heater for use in semiconductor wet chemical processing and method of manufacturing the same |
US7241131B1 (en) | 2000-06-19 | 2007-07-10 | Husky Injection Molding Systems Ltd. | Thick film heater apparatus |
US20080190912A1 (en) * | 2007-02-13 | 2008-08-14 | Wing Yiu Yeung | Heating Apparatus and Method for Making the Same |
US20100308955A1 (en) * | 2009-06-04 | 2010-12-09 | Cole Robert C | Ultra-Stable Refractory High-Power Thin Film Resistors for Space Applications |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5350969A (en) * | 1991-12-03 | 1994-09-27 | Litton Systems, Inc. | Cathode heater and cathode assembly for microwave power tubes |
CN1115705C (zh) * | 1996-05-21 | 2003-07-23 | 株式会社东芝 | 阴极组件、电子枪组件、电子管、灯丝、及阴极组件和电子枪组件的制造方法 |
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-
1990
- 1990-07-11 EP EP90307591A patent/EP0408342B1/fr not_active Expired - Lifetime
- 1990-07-11 DE DE69022651T patent/DE69022651D1/de not_active Expired - Lifetime
- 1990-07-11 US US07/550,976 patent/US5155340A/en not_active Expired - Fee Related
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Cited By (36)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5539186A (en) * | 1992-12-09 | 1996-07-23 | International Business Machines Corporation | Temperature controlled multi-layer module |
US5990449A (en) * | 1993-11-04 | 1999-11-23 | Pentel Kabushiki Kaisha | Electric heating device for mirror |
US5705272A (en) * | 1994-04-25 | 1998-01-06 | Canon Kabushiki Kaisha | Heating member and heat fixing apparatus using the same |
US5616423A (en) * | 1994-05-19 | 1997-04-01 | Sumitomo Metal Industries, Ltd. | Ceramic substrate having a multilayered metallic thin film |
US5569474A (en) * | 1994-06-06 | 1996-10-29 | Daiho Industrial Co., Ltd. | Mold for injection molding of plastics using thin film electric heater |
US5705793A (en) * | 1994-06-06 | 1998-01-06 | Daiho Industrial Co., Ltd. | Thin film electric heater, and method and apparatus for injection molding of plastics using the same |
US6575729B2 (en) | 1998-06-12 | 2003-06-10 | Husky Injection Molding Systems Ltd. | Molding system with integrated film heaters and sensors |
US6341954B1 (en) | 1998-06-12 | 2002-01-29 | Husky Injection Molding Systems Ltd. | Molding system using film heaters and/or sensors |
US20040222209A1 (en) * | 1998-06-12 | 2004-11-11 | Harold Godwin | Molding system with integrated film heaters and sensors |
US20030206991A1 (en) * | 1998-06-12 | 2003-11-06 | Harold Godwin | Molding system with integrated film heaters and sensors |
US7071449B2 (en) | 1998-06-12 | 2006-07-04 | Husky Injection Molding Systems Ltd. | Molding system with integrated film heaters and sensors |
US7029260B2 (en) | 1998-06-12 | 2006-04-18 | Husky Injection Molding Systems Ltd. | Molding apparatus having a film heater |
US20050129801A1 (en) * | 1998-06-12 | 2005-06-16 | Harold Godwin | Film heater apparatus and method for molding devices |
US6305923B1 (en) | 1998-06-12 | 2001-10-23 | Husky Injection Molding Systems Ltd. | Molding system using film heaters and/or sensors |
US6764297B2 (en) | 1998-06-12 | 2004-07-20 | Husky Injection Molding Systems Ltd. | Molding system with integrated film heaters and sensors |
US7241131B1 (en) | 2000-06-19 | 2007-07-10 | Husky Injection Molding Systems Ltd. | Thick film heater apparatus |
US6886233B2 (en) | 2002-05-13 | 2005-05-03 | Egc Enterprises, Inc. | Method for decreasing the thickness of flexible expanded graphite sheet |
US20040086449A1 (en) * | 2002-05-13 | 2004-05-06 | Rutherford Robert B. | Ultra-thin flexible expanded graphite resistance heater |
US6667100B2 (en) | 2002-05-13 | 2003-12-23 | Egc Enterprises, Inc. | Ultra-thin flexible expanded graphite heating element |
US7106167B2 (en) * | 2002-06-28 | 2006-09-12 | Heetronix | Stable high temperature sensor system with tungsten on AlN |
US7224256B2 (en) | 2002-06-28 | 2007-05-29 | Heetronix | Stable high temperature heater with serpentine heating strands on insulative substrate |
US20060267724A1 (en) * | 2002-06-28 | 2006-11-30 | Heetronix | Stable high temperature heater system with tungsten heating layer |
US20040056321A1 (en) * | 2002-06-28 | 2004-03-25 | Heetronix | Stable high temperature sensor system with tungsten on AlN |
US20060082433A1 (en) * | 2002-06-28 | 2006-04-20 | Heetronix | Stable high temperature with serpentine heating strands on insulative substrate |
US20040099047A1 (en) * | 2002-11-25 | 2004-05-27 | Raisanen Walfred R. | Thin film gas sensor |
US6786076B2 (en) * | 2002-11-25 | 2004-09-07 | Reliable Instruments Llc | Thin film gas sensor |
US6924468B2 (en) * | 2002-12-14 | 2005-08-02 | Thermoceramix, Inc. | System and method for heating materials |
US20040112892A1 (en) * | 2002-12-14 | 2004-06-17 | Abbott Richard C. | System and method for heating materials |
US20050274714A1 (en) * | 2004-06-14 | 2005-12-15 | Hongy Lin | In-line heater for use in semiconductor wet chemical processing and method of manufacturing the same |
US7164104B2 (en) * | 2004-06-14 | 2007-01-16 | Watlow Electric Manufacturing Company | In-line heater for use in semiconductor wet chemical processing and method of manufacturing the same |
US20080190912A1 (en) * | 2007-02-13 | 2008-08-14 | Wing Yiu Yeung | Heating Apparatus and Method for Making the Same |
US8193475B2 (en) * | 2007-02-13 | 2012-06-05 | Advanced Materials Enterprises Company Limited | Heating apparatus and method for making the same |
US20130140294A1 (en) * | 2007-02-13 | 2013-06-06 | Advanced Materials Enterprises Company Limited | Heating apparatus and method for making the same |
US8742303B2 (en) * | 2007-02-13 | 2014-06-03 | Advanced Materials Enterprises Company Limited | Heating apparatus and method for making the same |
US20100308955A1 (en) * | 2009-06-04 | 2010-12-09 | Cole Robert C | Ultra-Stable Refractory High-Power Thin Film Resistors for Space Applications |
US8284012B2 (en) * | 2009-06-04 | 2012-10-09 | The Aerospace Corporation | Ultra-stable refractory high-power thin film resistors for space applications |
Also Published As
Publication number | Publication date |
---|---|
EP0408342A2 (fr) | 1991-01-16 |
DE69022651D1 (de) | 1995-11-02 |
EP0408342A3 (en) | 1991-04-03 |
EP0408342B1 (fr) | 1995-09-27 |
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